JP2005097348A - Dispersion inkjet ink production method and inkjet recording method - Google Patents

Abstract

<P>PROBLEM TO BE SOLVED: To provide a dispersion inkjet ink production method and an inkjet recording method suitable as an inkjet textile printing image formation method (recording system) excellent in jettability and economy. <P>SOLUTION: The dispersion inkjet ink production method is a method for producing dispersion inkjet ink containing a colorant, a dispersant, water, and a water-soluble organic solvent, wherein the dissolved oxygen concentration in the dispersion inkjet ink is 2 ppm or lower after the dispersion inkjet ink is deaerated by using ultrasonic waves or a hollow fiber membrane before it is filled into a cartridge. <P>COPYRIGHT: (C)2005,JPO&NCIPI

Description

  The present invention relates to a method for producing a dispersed inkjet ink (hereinafter also referred to as inkjet ink, dispersion system ink, ink) and an inkjet recording method, and more particularly to a method for producing a dispersed inkjet ink for textile printing and an inkjet recording method.

  An ink jet image printing method is a method in which a minute droplet of ink is ejected and attached to a target medium for printing. The ink jet system is advantageous in that its mechanism is relatively simple and inexpensive, and can form high-definition and high-quality images.

  Utilizing the advantages of the ink jet system, printing on a fabric, that is, a so-called ink jet textile image forming method (recording system) has been developed.

  Unlike the conventional textile printing, the inkjet textile printing image forming method does not need to prepare a plate and can quickly form an image with excellent gradation. Further, since only an amount of ink necessary for an image is required, the image forming method is excellent in terms of environment such as a small amount of waste liquid.

  Therefore, there is a demand for an ink-jet printed image forming method capable of shortening the delivery time and responding to the production of a small variety of products.

  There are various types of ink jet recording methods, but the on-demand type recording methods which have become mainstream in recent years are the so-called piezo method (piezoelectric element method) using a piezo element and the thermal jet method (bubble jet (R) method). being classified. The piezo method is repeatedly pressed and depressurized many times during ink ejection, and micro bubbles are likely to be generated due to cavitation, causing dot dropout and landing position misalignment during ink ejection, and is known to degrade print quality such as graininess. ing.

  In general, cavitation is a physical phenomenon in which a liquid evaporates into bubbles when the pressure of the liquid at a certain temperature is lower than the vapor pressure determined by the temperature.

  The ink used for this purpose is usually deaerated, and the amount of gas contained in the ink is reduced as much as possible to prevent the generation of bubbles during ejection. As the degassing treatment, a method of degassing ink under reduced pressure, a method of irradiating ultrasonic waves, a method of using a degassing hollow fiber membrane described in JP-A-11-209670, and the like have been tried.

An apparatus incorporated in a printer has also been proposed in that ultrasonic deaeration and hollow fiber membrane deaeration can be performed continuously. Although not a physical method, Japanese Patent Application Laid-Open No. 11-263929 discloses that bubbles are generated by a surfactant. A prevention method has been proposed.

  However, although either method is sufficiently effective with dissolved ink, it is difficult to achieve stable emission by preventing cavitation in the case of dispersion ink.

  Furthermore, when incorporating in a printer, it is necessary to attach a deaeration device for each color of ink, and space is required, which increases the size of the printer and increases costs.

  In addition, the printer itself cannot be used in the event of a failure, and there are problems such as the occurrence of aggregates in the ink cartridge or in front of the deaeration device due to the gas contained in the ink when not used for a long time. .

A technique that improves the dispersibility by removing the adsorbed air on the pigment surface by using ultrasonic treatment and vacuum defoaming treatment to enhance the interaction with the dispersant has been proposed. It is not a thing. (For example, see Patent Document 1)
As described above, a dispersion ink satisfying stable emission and economy has not been obtained yet.
Japanese Patent Laid-Open No. 9-286943

  An object of the present invention is to provide a method for producing a dispersed inkjet ink and an inkjet recording method suitable for an inkjet printed image forming method (recording method) having excellent light emission properties and economy.

  The above object of the present invention is achieved by the following configurations.

  1. In a method for producing a dispersed inkjet ink containing a coloring material, a dispersant, water, and a water-soluble organic solvent, the dispersion inkjet ink is subjected to deaeration treatment with an ultrasonic wave and a hollow fiber membrane before filling the cartridge. A method for producing a dispersed inkjet ink, wherein the dissolved oxygen concentration in the dispersed inkjet ink is 2 ppm or less.

  2. 2. The method for producing a dispersed inkjet ink as described in 1 above, wherein the hollow fiber membrane is degassed and then subjected to ultrasonic treatment.

  3. 3. The method for producing a dispersed inkjet ink as described in 1 or 2 above, wherein the average particle size change of the disperse dye before and after the degassing treatment is within ± 5%.

  4). 4. The method for producing a dispersed inkjet ink according to any one of items 1 to 3, wherein the colorant is a disperse dye.

5). 5. The dispersion inkjet according to any one of 1 to 4, wherein the ultrasonic treatment is performed under conditions of an oscillation frequency of 10 to 30 kHz and an irradiation energy of 1 × 10 ⁴ to 1 × 10 ⁵ J. Ink manufacturing method.

  6). 6. An ink jet recording method comprising: recording an image with a dispersed inkjet ink obtained by the method for producing a dispersed inkjet ink according to any one of 1 to 5 above using an inkjet head having a nozzle diameter of 20 to 50 μm. .

  7). An image is recorded using a dispersion inkjet ink obtained by the method for producing a dispersion inkjet ink according to any one of 1 to 5 above on a fiber mainly composed of polyester having an ink receiving layer. Inkjet recording method.

  The method for producing a dispersed inkjet ink and the inkjet recording method of the present invention are suitable for an inkjet printed image forming method (recording method) excellent in light emission and economy and have excellent effects.

  The dispersed ink-jet ink of the present invention is an ink using a pigment or a disperse dye as a color material, and a known inorganic pigment, organic pigment, disperse dye or the like can be used.

  Examples of organic pigments include azo pigments such as azo lakes, insoluble azo pigments, condensed azo pigments, chelate azo pigments, phthalocyanine pigments, perylene and perylene pigments, anthraquinone pigments, quinacridone pigments, dioxazine pigments, thioindigo pigments, isoindolinone pigments, and quinophthalone pigments. Polycyclic pigments such as pigments, dye lakes such as basic dye type lakes and acid dye type lakes, nitro pigments, nitroso pigments, aniline black, daylight fluorescent pigments, and inorganic pigments such as carbon black Can be mentioned.

  Specific organic pigments are exemplified below.

  Examples of pigments for magenta or red include C.I. I. Pigment red 2, C.I. I. Pigment red 3, C.I. I. Pigment red 5, C.I. I. Pigment red 6, C.I. I. Pigment red 7, C.I. I. Pigment red 15, C.I. I. Pigment red 16, C.I. I. Pigment red 48: 1, C.I. I. Pigment red 53: 1, C.I. I. Pigment red 57: 1, C.I. I. Pigment red 122, C.I. I. Pigment red 123, C.I. I. Pigment red 139, C.I. I. Pigment red 144, C.I. I. Pigment red 149, C.I. I. Pigment red 166, C.I. I. Pigment red 177, C.I. I. Pigment red 178, C.I. I. And CI Pigment Red 222.

  Examples of the orange or yellow pigment include C.I. I. Pigment orange 31, C.I. I. Pigment orange 43, C.I. I. Pigment yellow 12, C.I. I. Pigment yellow 13, C.I. I. Pigment yellow 14, C.I. I. Pigment yellow 15, C.I. I. Pigment yellow 17, C.I. I. Pigment yellow 74, C.I. I. Pigment yellow 93, C.I. I. Pigment yellow 94, C.I. I. Pigment yellow 128, C.I. I. And CI Pigment Yellow 138.

  Examples of pigments for green or cyan include C.I. I. Pigment blue 15, C.I. I. Pigment blue 15: 2, C.I. I. Pigment blue 15: 3, C.I. I. Pigment blue 16, C.I. I. Pigment blue 60, C.I. I. And CI Pigment Green 7.

  As the disperse dye that can be preferably used in the present invention, various disperse dyes such as an azo disperse dye, a quinone disperse dye, an anthraquinone disperse dye, and a quinophthalone disperse dye can be used. Specific compound names are listed below, but the present invention is not limited thereto.

C. I. Disperse Yellow 3, 4, 5, 7, 9, 13, 23, 24, 30, 33, 34, 42, 44, 49, 50, 51, 54, 56, 58, 60, 63, 64, 66, 68, 71 74, 76, 79, 82, 83, 85, 86, 88, 90, 91, 93, 98, 99, 100, 104, 108, 114, 116, 118, 119, 122, 124, 126, 135, 140 141,149,160,162,163,164,165,179,180,182,183,184,186,192,198,199,202,204,210, 211,215,216,218,224,227 , 231,232
C. I. Disperse Orange 1, 3, 5, 7, 11, 13, 17, 20, 21, 25, 29, 30, 31, 32, 33, 37, 38, 42, 43, 44, 45, 46, 47, 48, 49 , 50, 53, 54, 55, 56, 57, 58, 59, 61, 66, 71, 73, 76, 78, 80, 89, 90, 91, 93, 96, 97, 119, 127, 130, 139 142,
C. I. Disperse Red 1, 4, 5, 7, 11, 12, 13, 15, 17, 27, 43, 44, 50, 52, 53, 54, 55, 56, 58, 59, 60, 65, 72, 73, 74 75, 76, 78, 81, 82, 86, 88, 90, 91, 92, 93, 96, 103, 105, 106, 107, 108, 110, 111, 113, 117, 118, 121, 122, 126 127,128,131,132,134,135,137,143,145,146,151,152,153,154,157,159,164,167,169,177,179,181,183,184,185 , 188, 189, 190, 191, 192, 200, 201, 202, 203, 205, 206, 207, 210, 221, 224, 225 , 227, 229, 239, 240, 257, 258, 277, 278, 279, 281, 288, 298, 302, 303, 310, 311, 312, 320, 324, 328,
C. I. Disperse Violet 1, 4, 8, 23, 26, 27, 28, 31, 33, 35, 36, 38, 40, 43, 46, 48, 50, 51, 52, 56, 57, 59, 61, 63, 69 , 77,
C. I. Disperse Green9
C. I. Disperse Brown 1, 2, 4, 9, 13, 19
C. I. Disperse Blue 3, 7, 9, 14, 16, 19, 20, 26, 27, 35, 43, 44, 54, 55, 56, 58, 60, 62, 64, 71, 72, 73, 75, 79, 81 , 82, 83, 87, 91, 93, 94, 95, 96, 102, 106, 108, 112, 113, 115, 118, 120, 122, 125, 128, 130, 139, 141, 142, 143, 146 , 148, 149, 153, 154, 158, 165, 167, 171, 173, 174, 176, 181, 183, 185, 186, 187, 189, 197, 198, 200, 201, 205, 207, 211, 214 , 224, 225, 257, 259, 267, 268, 270, 284, 285, 287, 288, 291, 293, 295, 2 97, 301, 315, 330, 333,
C. I. Disperse Black 1, 3, 10, 24
Etc.

  The disperse dye content is preferably 3 to 20% by mass, more preferably 5 to 13% by mass.

  The disperse dye may be used as a commercial product, but it is preferable to carry out a purification treatment. As a purification method, a known recrystallization method, washing or the like can be used. The organic solvent used in the purification method and purification treatment is preferably selected as appropriate according to the type of dye.

  Examples of the dispersant preferably used in the present invention include, for example, formalin condensate of sodium creosote oil sulfonate (eg, demole C), formalin condensate of sodium cresol sulfonate and sodium 2-naphthol-6-sulfonate, cresol sulfone. Formalin condensate of sodium acid salt, formalin condensate of sodium phenol sulfonate, formalin condensate of sodium β-naphthol sulfonate, formalin condensate of sodium β-naphthalene sulfonate (eg demole N) and sodium β-naphthol sulfonate, Examples include lignin sulfonate (for example, Vanillex RN), sodium paraffin sulfonate (for example, Efcol 214), and a copolymer of α-olefin and maleic anhydride (for example, Florene G-700). Lignin sulfonic acid salt is preferred.

  As for the usage-amount of a dispersing agent, 20-200 mass% is preferable with respect to a disperse dye. When the amount of the dispersant is small, the formation of fine particles and the dispersion stability are poor. These dispersants may be used alone or in combination.

  Depending on the structure of the disperse dye used, foaming or gelation may occur during dispersion, resulting in poor fluidity. In addition to the ability to form fine particles and dispersion stability, foaming during dispersion and gelation of the dispersion It is necessary to select in consideration of the fluidity of the dispersion. An antifoaming agent may be added to improve foaming during dispersion. In addition, the dispersant can affect the dyeability, dyeing rate, leveling property, transferability, color tone, fastness, etc. of the fabric, and tar of the dispersant or wetting agent when coloring at high temperatures. It is preferable to select in consideration of the fact that the dyeing becomes non-uniform due to the conversion.

  Since there is no dispersant that satisfies all of the above requirements, it is necessary to select an optimal dispersant according to the dye to be dispersed and add an antifoaming agent or the like as necessary.

  Examples of the water-soluble organic solvent preferably used in the present invention include polyhydric alcohols (for example, ethylene glycol, glycerin, 2-ethyl-2- (hydroxymethyl) -1,3-propanediol, tetraethylene glycol, triethylene glycol). Ethylene glycol, tripropylene glycol, 1,2,4-butanetriol, diethylene glycol, propylene glycol, dipropylene glycol, butylene glycol, 1,6-hexanediol, 1,2-hexanediol, 1,5-pentanediol, 1 , 2-pentanediol, 2,2-dimethyl-1,3-propanediol, 2-methyl-2,4-pentanediol, 3-methyl-1,5-pentanediol, 3-methyl-1,3-butane Diol, 2-methyl-1,3-propanedio Etc.), amines (eg ethanolamine, 2- (dimethylamino) ethanol etc.), monohydric alcohols (eg methanol, ethanol, butanol etc.), polyhydric alcohol alkyl ethers (eg diethylene glycol monomethyl ether, Diethylene glycol monobutyl ether, triethylene glycol monomethyl ether, triethylene glycol monobutyl ether, ethylene glycol monomethyl ether, ethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol monobutyl ether, dipropylene glycol monomethyl ether, etc.), 2,2'-thio Diethanol, amides (for example, N, N-dimethylformamide and the like), heterocyclic rings (2-pyrrolidone and the like), Acetonitrile, and the like.

  The amount of the water-soluble organic solvent is preferably 10 to 60% by mass with respect to the total ink mass.

  The particle size of the disperse dye is preferably 300 nm or less as the average particle size and 900 nm or less as the maximum particle size. When the average particle size and the maximum particle size exceed 300 nm and 900 nm, respectively, clogging is likely to occur in the ink jet printing method in which light is emitted from a fine nozzle, and stable emission cannot be performed.

  The average particle size can be determined by a commercially available particle size measuring device using a light scattering method, an electrophoresis method, a laser Doppler method, or the like. Specific examples of the particle diameter measuring apparatus include Zetar Sizer 1000 manufactured by Malvern.

  When measured with Malter Zeta Sizer 1000, it can be said that there is no difference in the average particle diameter within ± 5% considering the measurement accuracy.

  Furthermore, additives can be used to improve various performances. As the additive, known antiseptics, antifungal agents, viscosity modifiers, metal chelating agents, antioxidants, ultraviolet absorbers and the like can be used.

For the long-term storage stability of the ink, preservatives and antifungal agents may be added. As preservatives and antifungal agents, aromatic halogen compounds, methylene dithiocyanates, halogen-containing nitrogen sulfur compounds, 1,2- Examples include benzisothiazolin-3-one, but the present invention is not limited thereto.

  The dispersion inkjet ink is dispersed in an aqueous dispersion medium at a high concentration by using a dispersion apparatus such as a ball mill, a sand mill, a roll mill, a speed line mill, a homomixer, or a sand grinder. It can be manufactured by diluting about twice, adding various additives, converting it to ink, degassing treatment, and filtering.

  The present invention is characterized by degassing by performing ultrasonic treatment and hollow fiber membrane treatment before filling the cartridge with the dispersed inkjet ink, and the oxygen concentration in the dispersed inkjet ink after the degassing treatment is 2 ppm. By making the following, stable emission could be achieved.

  It should be noted that it has been difficult to achieve stable emission even if each of the deaeration operations already performed and proposed is performed alone.

  However, as a result of various studies, the present inventor has found that the object of the present invention can be achieved by performing deaeration by ultrasonic treatment and hollow fiber membrane treatment.

  Furthermore, it has also been found that performing the deaeration process first using a hollow fiber membrane and then performing the deaeration process by ultrasonic treatment has the greatest effect of the present invention.

  Although its action and mechanism are not clear, it is estimated as follows.

  First, by performing a deaeration process using a hollow fiber membrane, the gas dissolved in the ink and the microbubbles (called bubble nuclei) present in the solvent are removed.

  However, the surface of the dispersed ink is not completely covered with the dispersant, and minute bubbles (bubble nuclei) are attached.

  Therefore, it is presumed that when ultrasonic treatment is performed and vibration is applied, bubble nuclei are detached from the surface of the dispersed ink, accumulate and float on the gas-liquid interface or dissolve in the solvent, and the bubbles disappear.

  Before and after these degassing treatments, no change in particle size was observed, so dispersibility was improved, and the output performance was not improved. Gas in the ink was sufficiently removed, and cavitation was not generated during head ejection. It is estimated that stable emission has become possible.

  A commercially available deaeration module for deaeration treatment using the hollow fiber membrane of the present invention can be used. For example, Mitsubishi Rayon Co., Ltd. MHF series, Dainippon Ink & Chemicals, Inc. SEPAREL series, etc. are mentioned.

  The deaeration process using the hollow fiber membrane module is performed, for example, by supplying ink from the ink supply port at the end of the module to the inside of the hollow fiber membrane and sucking it from the gas deaeration port on the side wall of the module. While the pressure is reduced as described below, the dissolved gas in the ink that has passed through the membrane is discharged, and the deaerated ink exits from the ink outlet at the other end of the module. In the deaeration process using the hollow fiber membrane module, ink can be supplied to the outside of the hollow fiber membrane and the inside can be decompressed.

Although the apparatus used for the ultrasonic treatment of the present invention is not particularly limited, it is manufactured by Nippon Seiki Seisakusho Co., Ltd. Circulation type RUS-600TCVP (frequency 20 kHz, maximum output 600 W), Branson Co., Ltd. continuous model 900 type (frequency 20 kHz, Ultrasonic treatment conditions include frequency, amplitude, and irradiation energy. If the frequency is higher than 30 KHz, the cohesive action becomes stronger and the dispersibility deteriorates, so the range is from 10 to 30 kHz. Since the cavitation pressure is higher as the amplitude is larger, the general amplitude range is 20 to 60 μm, and the irradiation energy is preferably 1 × 10 ⁴ to 1 × 10 ⁵ J, more preferably 2 × 10 ^4. ~ 8x10 ⁴ J.

If the irradiation energy is less than 1 × 10 ⁴ J, the ability to remove bubble nuclei is insufficient, and if it exceeds 1 × 10 ⁵ J, the temperature rises and causes aggregation.

  In addition, ultrasonic deaeration may be performed after the deaeration process using the hollow fiber membrane is once stored in a kettle or the like, but it is preferable to perform the deaeration continuously.

  The dissolved oxygen concentration in the ink can be measured by the Ostwald method (experimental chemistry course 1 basic operation [I], page 241, 1975, Maruzen), the mass spectrum method, the galvanic cell type, the polarographic type, etc. It can be measured with a simple oxygen concentration meter or colorimetric analysis.

As a commercially available dissolved oxygen concentration meter (Toa Denpa Kogyo Co., Ltd. DO-30A type) can be mentioned.

  If the dissolved oxygen concentration exceeds 2 ppm, cavitation occurs when ink is ejected. Therefore, it is preferably less than 1 ppm, and more preferably less than 1 ppm. 0 ppm is particularly preferred.

  In order to obtain a high-definition image, recording is preferably performed using an inkjet head having a nozzle diameter of 10 μm to 50 μm. From the viewpoint of graininess, the upper limit is preferably 50 μm or less, and the lower limit is preferably 10 μm or more because the droplet volume becomes too small and is affected by airflow.

  The fabric preferably used in the present invention is preferably a fabric mainly composed of polyester fibers. Fibers mainly composed of polyester fibers may be made into any form such as woven fabric, knitted fabric, and non-woven fabric. The fabric is preferably 100% polyester fiber, but a blended woven fabric or a blended non-woven fabric with rayon, silk, polyurethane, acrylic, nylon, wool, or the like can also be used. Further, the thickness of the yarn constituting the fabric as described above is preferably in the range of 10 to 100d.

  In the ink jet recording method for textile printing of the present invention, it is preferable to pretreat the ink receiving layer to prevent image bleeding. As the pretreatment, a method in which 0.2 to 50% by mass of at least one substance such as a water-soluble polymer, a water-soluble metal salt, a polycation compound, a surfactant, and a water repellent can be used. It is preferable to use a method suitable for the fiber material.

As the water-soluble metal salt, an inorganic salt such as an alkali metal atom such as KCl or CaCl ₂ or an alkaline earth metal, an organic acid salt, or the like is preferably used.

  As the polycation compound, polymers or oligomers of various quaternary ammonium salts, polyamine salts, and the like can be used.

  Some water-soluble metal salts and polycation compounds change the color tone of the dyed product or reduce the light fastness, and therefore are preferably selected according to the target dyed product.

  Examples of water-soluble polymers include natural polymers (for example, starches such as corn and wheat, cellulose derivatives such as carboxymethylcellulose, methylcellulose, and hydroxyethylcellulose, sodium alginate, guar gum, tamarind gum, locust bean gum, gum arabic, etc. Polysaccharides, proteins such as gelatin, casein, keratin, etc.) and synthetic polymers (for example, polyvinyl alcohol, polyvinyl pyrrolidone, acrylic acid polymers, etc.) can be used.

  As the surfactant, for example, anionic, cationic, amphoteric, and nonionic surfactants are used. Typically, anionic surfactants include higher alcohol sulfates, sulfonates of naphthalene derivatives, and the like. Quaternary surfactants include quaternary ammonium salts, amphoteric surfactants such as imidazolidine derivatives, and nonionic surfactants include polyoxyethylene alkyl ethers, polyoxyethylene propylene block polymers, sorbitan fatty acids. Examples include esters, polyoxyethylene sorbitan fatty acid esters, and ethylene oxide adducts of acetylene alcohol.

  Examples of the water repellent include silicon, fluorine-based and wax-based ones.

  These water-soluble polymers and surfactants that are preliminarily applied to the fabric are stable against high-temperature environments because they do not cause stains due to tarring and the like when ink-jet printing and color development at high temperatures. It is preferable. Also, these water-soluble polymers and surfactants that are previously applied to the fabric. What is easy to remove from a cloth by the washing | cleaning process after carrying out inkjet printing and making it color at high temperature is preferable.

  Moreover, a carrier can also be provided to the fabric from the viewpoint of dyeability. The compound used as a carrier is preferably a compound having characteristics such as large dyeing acceleration, simple use, stable, low burden on human body and environment, easy removal from fibers, and no influence on dye fastness. . Examples of the carrier include phenols such as o-phenylphenol, p-phenylphenol, methylnaphthalene, alkyl benzoate, alkyl salicylate, chlorobenzene and diphenyl, ethers, organic acids, hydrocarbons and the like. These promote the swelling and plasticization of fibers such as polyester, and have a function of making the disperse dye easily enter the fibers.

  In addition, a dyeing assistant can be added to the fabric. The dyeing assistant has the effect of reducing the amount of moisture that re-evaporates and shortening the temperature rising time by forming a eutectic compound with water aggregated on the fabric when steaming the printed fabric. Further, this eutectic compound has a function of dissolving the dye on the fiber and promoting the diffusion rate of the dye into the fiber. Urea is mentioned as a dyeing assistant.

  The pretreatment agent is preferably selected according to the fabric material and fabric structure, and is preferably applied by a pad method, a coating method, a spray method or the like so as to contain 0.2 to 50% by mass in the fabric. In the textile printing method of the present invention, after forming an image by the ink jet recording method on the fabric containing the fiber that can be dyed with the disperse dye as described above (ink application) Step), the fabric to which the ink is applied is heat-treated (heat treatment step), and further, the fabric subjected to the heat treatment is washed (washing step), whereby the printing on the fabric is completed and a printed matter is obtained. In the textile printing method of the present invention, the disperse dye is fixed to the fiber by a method of heat-treating a fabric to which ink is applied. Furthermore, as a method for removing unfixed dye from the fabric, a conventionally known cleaning method can be used, but it is particularly preferable to use a reduction cleaning.

  In the ink jet textile printing method for printing on a cloth, it is desirable to wind up the printed cloth after emitting the ink, develop a color by heating, and wash and dry the cloth. In ink jet textile printing, ink is printed on a fabric and simply left unattended, it does not dye well. In addition, when printing on a long fabric for a long time, the fabric comes out endlessly, and the printed fabric overlaps with the floor, etc., and it is unsafe and unexpectedly dirty. There is a case. Therefore, it is necessary to perform a winding operation after printing. During this operation, a medium not related to printing, such as paper, cloth, or vinyl, may be sandwiched between the cloths. However, it is not always necessary to wind up when cutting in the middle or short fabric.

  The printed fabric may be immediately heat-treated or may be heat-treated after a while, and may be dried and colored according to the intended use. As the heat treatment method, a method suitable for the application, such as an oven, a heat roll, or steam, may be selected.

  Cleaning is necessary after heat treatment. This is because a dye that has not participated in the dyeing remains, resulting in poor color stability and low fastness. It is also necessary to remove the pretreatment product applied to the fabric. If left as it is, the fabric is dyed as well as a decrease in fastness. Therefore, cleaning according to the object to be removed and the purpose is necessary.

  Drying is required after washing. After the washed fabric is squeezed or dehydrated, it is dried or dried using a dryer, heat roll, iron or the like.

  In addition, in order to obtain a uniform dyed product, the ink jet recording method of the present invention has natural impurities (oils, waxes, pectic substances, natural pigments, etc.) adhering to the fabric fibers before the ink receiving layer is pretreated on the fabric. In addition, it is desirable to wash away residues (such as glue) and dirt used in the fabric manufacturing process. As cleaning agents used for cleaning, alkalis such as sodium hydroxide and sodium carbonate, surfactants such as anionic surfactants and nonionic surfactants, enzymes and the like are used.

  By this series of actions, the characteristics of the dispersed ink-jet ink for printing of the present invention are utilized, and a fabric on which a beautiful pattern is printed is completed.

  EXAMPLES Hereinafter, although an Example is given and this invention is demonstrated concretely, the embodiment of this invention is not limited to these.

Example 1
[Dye purification]
A commercially available disperse thread 302 was suspended and stirred in refluxing methanol, filtered and dried, further recrystallized from ethyl acetate and dried to purify the dye.

[Preparation of dispersion ink]
Dispersion-1
The following mixture was dispersed using a sand grinder. Dispersion stopped when the average particle size reached 160 nm.

Commercial C.I. I. Disperse Red 302 30 parts Glycerin 10 parts Ion exchange water 30 parts Sodium lignin sulfonate 30 parts (Vanilex RN Nippon Paper Industries Co., Ltd.)
Further, the following components were mixed and then filtered through a 0.3 μm membrane filter to prepare a dispersion ink.

Dispersion liquid-1 20 parts Ethylene glycol 20 parts Glycerin 10 parts Proxel GXL (D) 0.01 part (manufactured by Avicia Co., Ltd.)
Ion-exchanged water 50 parts [Deaeration treatment]
Ultrasonic homogenizer manufactured by Nihon Seiki Seisakusho Co., Ltd. Ultrasonic homogenizer Circulation type RUS-600TCVP (frequency 20 kHz, output 600 W), irradiation energy 3.6 × 10 ⁴ J, (600 W for 1 minute / 1 L ink), flow rate 60 L 1 pass at / h.

  Subsequently, deaeration treatment was performed at 10 kPa or less with a hollow fiber membrane module (SEPAREL PF-004D manufactured by Dainippon Ink and Chemicals, Inc.).

  The ink after the above treatment was filled in an ink cartridge to obtain dispersion ink-1.

[Measurement of average particle size of disperse dye]
The dispersed ink after the first deaeration treatment and after the last deaeration treatment were sampled, and each was measured five times by the scattering intensity distribution measurement of Malter Zeta Sizer 1000, and the average value was taken.

[Measurement of oxygen concentration (DO value) in ink solution]
Before the first deaeration treatment, the ink after the last deaeration treatment was sampled and measured at 25 ° C. and 101 kpa using a solution oxygen analyzer (DO-30A type manufactured by Toa Denpa Kogyo Co., Ltd.).

[Outgoing light evaluation 1]
Using a piezo-type head having a nozzle diameter of 50 μm, a driving frequency of 10 kHz, and the number of nozzles of 64, the emission was evaluated. The drive voltage was adjusted so that each ink volume was 60 pL.

(Stable emission)
In an environment of 25 ° C. and a relative humidity of 50%, 500 ml of each ink was continuously discharged, and bending and non-occurrence that occurred until the ink ran out were evaluated according to the following evaluation criteria.

A: All nozzles emitted: B: 1-3 nozzles are bent and missing.

  (Triangle | delta): It curves with 4-7 nozzles, and a failure is seen.

  X: Bending is observed at 8 to 12 nozzles, and missing is observed.

  XX: Bending at 13 nozzles or more, and missing.

[Outgoing evaluation 2]
Using a piezo-type head having a nozzle diameter of 30 μm, a driving frequency of 20 kHz, and the number of nozzles of 64, the emission was performed and the emission performance was evaluated. The drive voltage was adjusted so that each ink volume was 20 pL.

(Stable emission)
In the environment of 25 ° C. and 50% relative humidity, 500 ml of each ink is continuously ejected, and bending and non-occurrence that occur until the ink runs out are evaluated according to the following evaluation criteria.

A: All nozzles emitted: B: 1-3 nozzles are bent and missing.

  (Triangle | delta): It curves with 4-7 nozzles, and a failure is seen.

  X: Bending is observed at 8 to 12 nozzles, and missing is observed.

  XX: Bending at 13 nozzles or more, and missing.

[Ejectivity evaluation 3 (preservation evaluation)]
The ink was filled in the cartridge and allowed to stand at 40 ° C. for 2 weeks.

[Processing before and after fabric]
A 100% polyester fiber and a thread thickness of 50d were previously immersed in a pretreatment agent (polymer cation compound and guar gum), squeezed and dried. After printing, the fabric was heat-treated at 180 ° C. for 10 minutes, washed with water and dried.

[Graininess evaluation]
A gradation chart having a halftone dot percentage of 0% to 100% was printed with an inkjet printing printer Nassenger II KS-1600II manufactured by Konica Corporation, and the graininess was visually evaluated. A piezo head with a nozzle diameter of 30 μm was used for printing.

Evaluated according to the following criteria: A: There is no roughness in the entire gradation.

  ○: Roughness is felt in the low concentration region.

  X: There is a feeling of roughness.

Example 2
A dispersion ink was prepared in the same manner as in Example 1.

[Deaeration treatment]
The dispersion ink was degassed at 10 kPa or less using a hollow fiber membrane module (SEPAREL PF-004D manufactured by Dainippon Ink and Chemicals, Inc.).
Continuously Ultrasonic homogenizer manufactured by Nippon Seiki Seisakusho Co., Ltd. Circulation type RUS-600TCVP (frequency 20 kHz, output 600 W), irradiation energy 3.6 × 10 ⁴ J, (600 W for 1 minute / 1 L ink), flow rate 60 L / h 1 pass processing.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Example 3
A dispersion ink was prepared in the same manner as in Example 1.

[Deaeration treatment]
The dispersion ink was degassed at 10 kPa or less using a hollow fiber membrane module (SEPAREL PF-004D manufactured by Dainippon Ink and Chemicals, Inc.).
Continuously Ultrasonic homogenizer manufactured by Nippon Seiki Seisakusho Co., Ltd. Circulation type RUS-600TCVP (frequency 20 kHz, output 600 W), irradiation energy 7.2 × 10 ⁴ J (600 W for 2 minutes / 1 L ink), flow rate 60 L / h One pass was processed.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Example 4
[Dye purification]
Commercially available Disperse Blue 60 was suspended and stirred with refluxing acetonitrile, filtered and dried, further recrystallized with ethyl acetate and dried to purify the dye.

[Preparation of dispersion]
Dispersion 2
The following mixture was dispersed using a sand grinder. Dispersion stopped when the average particle size reached 180 nm.

Commercial C.I. I. Disperse Blue 60 30 parts Glycerin 10 parts Ion-exchanged water 30 parts Creosote oil sodium sulfonate 30 parts (Demol C Kao Co., Ltd.)
Further, the following components were mixed with a 0.3 μm membrane filter to obtain an ink.

Dispersion-2-20 parts Ethylene glycol 20 parts Glycerin 10 parts Proxel GXL (D) 0.01 part (Avisia Co., Ltd.)
Deionized water 50 parts Deaeration treatment was performed in the same manner as in Example 1.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Example 5
A dispersion ink was prepared in the same manner as in Example 4. The deaeration treatment was performed in the same manner as in Example 2.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Example 6
A dispersion ink was prepared in the same manner as in Example 4. The deaeration treatment was performed in the same manner as in Example 3.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Comparative Example 1
A dispersion ink was prepared in the same manner as in Example 1. The deaeration treatment was performed by vacuum degassing the ink at 700 mmHg for 1 hour. Measurement of average particle diameter, measurement of dissolved oxygen concentration, evaluation of emissivity 1-3, before and after the fabric Processing and graininess evaluation were performed in the same manner as in Example 1.

Comparative Example 2
A dispersion ink was prepared in the same manner as in Example 1. [Deaeration treatment]
The dispersion ink was degassed at 10 kPa or less using a hollow fiber membrane module (SEPAREL PF-004D manufactured by Dainippon Ink and Chemicals, Inc.).

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Comparative Example 3
A dispersion ink was prepared in the same manner as in Example 1. [Deaeration treatment]
Ultrasonic homogenizer manufactured by Nihon Seiki Seisakusho Co., Ltd. Ultrasonic homogenizer Circulation type RUS-600TCVP (frequency 20 kHz, output 600 W), irradiation energy 3.6 × 10 ⁴ J, (600 W for 1 minute / 1 L ink), flow rate 60 L 1 pass at / h.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Comparative Example 4
A dispersion ink was prepared in the same manner as in Example 1. [Deaeration treatment]
The ink was vacuum degassed at 700 mmHg for 1 hour, followed by irradiation energy of 3.6 × 10 ⁴ J, (600 W) using an ultrasonic homogenizer circulation type RUS-600TCVP (frequency 20 kHz, output 600 W) manufactured by Nippon Seiki Seisakusho. 1 minute / 1L ink)
1 pass treatment at a flow rate of 60 L / h.

  The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

Comparative Example 5
A dispersion ink was prepared in the same manner as in Example 4. [Deaeration treatment]
The ink was vacuum degassed at 700 mmHg for 1 hour, followed by irradiation energy of 3.6 × 10 ⁴ J, (600 W) using an ultrasonic homogenizer circulation type RUS-600TCVP (frequency 20 kHz, output 600 W) manufactured by Nippon Seiki Seisakusho. 1 minute / 1L ink)
The measurement of the average particle diameter, the measurement of the dissolved oxygen concentration, the emissivity evaluations 1 to 3, the pre- and post-treatments of the fabric, and the granularity evaluation were performed in the same manner as in Example 1.

  The results are shown below.

  As can be seen from the table, the examples of the present invention are superior to the comparative examples.

Claims (7)

In a method for producing a dispersed inkjet ink containing a coloring material, a dispersant, water, and a water-soluble organic solvent, the dispersion inkjet ink is subjected to deaeration treatment with an ultrasonic wave and a hollow fiber membrane before filling the cartridge. A method for producing a dispersed inkjet ink, wherein the dissolved oxygen concentration in the dispersed inkjet ink is 2 ppm or less. The method for producing a dispersed inkjet ink according to claim 1, wherein a deaeration process using the hollow fiber membrane is performed, followed by an ultrasonic process. The method for producing a dispersed inkjet ink according to claim 1 or 2, wherein the average particle size change of the disperse dye before and after the degassing treatment is within ± 5%. The method for producing a dispersed inkjet ink according to claim 1, wherein the colorant is a disperse dye. The dispersion system according to any one of claims 1 to 4, wherein the ultrasonic treatment is performed under conditions of an oscillation frequency of 10 to 30 kHz and an irradiation energy of 1 x 10 ⁴ to 1 x 10 ⁵ J. A method for producing an inkjet ink. An inkjet recording using an inkjet head having a nozzle diameter of 20 to 50 μm and recording an image with the dispersed inkjet ink obtained by the method for producing a dispersed inkjet ink according to claim 1. Method. An image is recorded on a fiber mainly composed of polyester having an ink receiving layer, using the dispersed inkjet ink obtained by the method for producing a dispersed inkjet ink according to any one of claims 1 to 5. An inkjet recording method.